scholarly journals In Search of Factors Determining Activity of Co3O4 Nanoparticles Dispersed in Partially Exfoliated Montmorillonite Structure

Molecules ◽  
2021 ◽  
Vol 26 (11) ◽  
pp. 3288
Author(s):  
Anna Rokicińska ◽  
Tomasz Berniak ◽  
Marek Drozdek ◽  
Piotr Kuśtrowski

The paper discusses a formation of Mt–PAA composite containing a natural montmorillonite structure partially exfoliated by poly(acrylic acid) introduced through intercalation polymerization of acrylic acid. Mt–PAA was subsequently modified by controlled adsorption of Co2+ ions. The presence of aluminosilicate packets (clay) and carboxyl groups (hydrogel) led to the deposition of significant amounts of Co2+ ions, which after calcination formed the Co3O4 spinel particles. The conditions of the Co2+ ions’ deposition (pH, volume and concentration of Co(NO3)2 solution, as well as a type of pH-controlling agent) were widely varied. Physicochemical characterization of the prepared materials (including X-ray fluorescence (XRF), X-ray powder diffraction (XRD), low-temperature nitrogen adsorption, X-ray photoelectron spectroscopy (XPS) and temperature-programmed reduction (H2-TPR)) revealed that the modification conditions strongly influenced the content as well as the distribution of the Co3O4 active phase, tuning its reducibility. The latter parameter was, in turn, very important from the point of view of catalytic activity in the combustion of aromatic volatile organic compounds (VOCs) following the Mars–van Krevelen mechanism.

Processes ◽  
2021 ◽  
Vol 9 (11) ◽  
pp. 1925
Author(s):  
Tao Yu ◽  
Zhuo Chen ◽  
Yundong Wang ◽  
Jianhong Xu

H2S is a common but hazardous impurity in syngas, biogas, or natural gas. For some advanced power generation technologies, such as integrated gasification combined cycle (IGCC), solid oxide fuel cells, H2S content needs to be reduced to an acceptable level. In this work, a series of highly porous Zn-Cu and Zn-Co composites with three-dimensionally ordered macropores (3DOM) structure were synthesized via the colloidal crystal template method and used to remove H2S at 150 °C and one atm. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), nitrogen adsorption studies, X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) were carried out to analyze the fresh and spent adsorbents. The results show that all the adsorbents possess well-ordered macropores, a large surface area, and a highly dispersed active phase. The relative content of Zn and (Cu or Co) has a significant influence on the desulfurization performance of adsorbents. The addition of CuO significantly increases the sulfur capacity and 3DOM-Zn0.5Cu0.5 shows the largest sulfur capacity of all the adsorbents, reaching up to 102.5 mg/g. The multiple adsorption/regeneration cycles of 3DOM-Zn0.5Cu0.5 and 3DOM-Zn0.5Co0.5 indicate that the as-prepared adsorbents are stable, and the sulfur capacity can still exceed 65% of the fresh adsorbents after six cycles.


Nanomaterials ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 1519
Author(s):  
Jong Gyeong Kim ◽  
Sunghoon Han ◽  
Chanho Pak

The price and scarcity of platinum has driven up the demand for non-precious metal catalysts such as Fe-N-C. In this study, the effects of phosphoric acid (PA) activation and phosphorus doping were investigated using Fe-N-C catalysts prepared using SBA-15 as a sacrificial template. The physical and structural changes caused by the addition of PA were analyzed by nitrogen adsorption/desorption and X-ray diffraction. Analysis of the electronic states of Fe, N, and P were conducted by X-ray photoelectron spectroscopy. The amount and size of micropores varied depending on the PA content, with changes in pore structure observed using 0.066 g of PA. The electronic states of Fe and N did not change significantly after treatment with PA, and P was mainly found in states bonded to oxygen or carbon. When 0.135 g of PA was introduced per 1 g of silica, a catalytic activity which was increased slightly by 10 mV at −3 mA/cm2 was observed. A change in Fe-N-C stability was also observed through the introduction of PA.


2020 ◽  
Vol 2020 ◽  
pp. 1-9 ◽  
Author(s):  
N. Cruz-González ◽  
O. Calzadilla ◽  
J. Roque ◽  
F. Chalé-Lara ◽  
J. K. Olarte ◽  
...  

In the last decade, the urgent need to environmental protection has promoted the development of new materials with potential applications to remediate air and polluted water. In this work, the effect of the TiO2 thin layer over MoS2 material in photocatalytic activity is reported. We prepared different heterostructures, using a combination of electrospinning, solvothermal, and spin-coating techniques. The properties of the samples were analyzed by scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), X-ray diffraction (XRD), nitrogen adsorption-desorption isotherms, UV-Vis diffuse reflectance spectroscopy (UV-Vis-DRS), and X-ray photoelectron spectroscopy (XPS). The adsorption and photocatalytic activity were evaluated by discoloration of rhodamine B solution. The TiO2-MoS2/TiO2 heterostructure presented three optical absorption edges at 1.3 eV, 2.28 eV, and 3.23 eV. The high adsorption capacity of MoS2 was eliminated with the addition of TiO2 thin film. The samples show high photocatalytic activity in the visible-IR light spectrum.


2010 ◽  
Vol 75 ◽  
pp. 36-42 ◽  
Author(s):  
Marina Rumyantseva ◽  
Irina Zhurbina ◽  
Elena Varechkina ◽  
Siranuysh Badalyan ◽  
Alexander Gaskov ◽  
...  

Powders of tin dioxide (SnO2) have been prepared by two different modifications of wet chemical synthesis, i.e. (i) by conventional hydrolysis of tin chloride dissolved in aqueous ammonia solution and (ii) by precipitation from tin chloride dissolved in aqueous hydrazine monohydrate (N2H4*H2O) solution. The prepared gels were dried and then annealed at different temperatures varied from 300 to 700 oC in order to form nanocrystals. Structure and optical properties of the samples were investigated by using X-ray diffraction, transmission electron microscopy, thermoprogrammable hydrogen reduction, low temperature nitrogen adsorption method, photoluminescence, infra-red absorption, Raman spectroscopy, and X-ray photoelectron spectroscopy. The samples prepared by hydrazine-based method are characterized by surface area about 127-188 m2/g with high sintering resistance. The optical spectroscopy data revealed pure crystallinity and high defect concentration for the samples prepared by hydrazine-based method. The experimental results are discussed in view of different states of chemisorbed oxygen on SnO2 nanocrystal surfaces, which determine electronic and optical properties of the prepared samples.


2019 ◽  
Vol 2019 ◽  
pp. 1-15 ◽  
Author(s):  
Pham Dinh Du ◽  
Huynh Thi Minh Thanh ◽  
Thuy Chau To ◽  
Ho Sy Thang ◽  
Mai Xuan Tinh ◽  
...  

In the present paper, the synthesis of metal-organic framework MIL-101 and its application in the photocatalytic degradation of Remazol Black B (RBB) dye have been demonstrated. The obtained samples were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS), and nitrogen adsorption/desorption isotherms at 77 K. It was found that MIL-101 synthesized under optimal conditions exhibited high crystallinity and specific surface area (3360 m2·g-1). The obtained MIL-101 possessed high stability in water for 14 days and several solvents (benzene, ethanol, and water at boiling temperature). Its catalytic activities were evaluated by measuring the degradation of RBB in an aqueous solution under UV radiation. The findings show that MIL-101 was a heterogeneous photocatalyst in the degradation reaction of RBB. The mechanism of photocatalysis was considered to be achieved by the electron transfer from photoexcited organic ligands to metallic clusters in MIL-101. The kinetics of photocatalytic degradation reaction were analyzed by using the initial rate method and Langmuir-Hinshelwood model. The MIL-101 photocatalyst exhibited excellent catalytic recyclability and stability and can be a potential catalyst for the treatment of organic pollutants in aqueous solutions.


Materials ◽  
2019 ◽  
Vol 12 (11) ◽  
pp. 1771 ◽  
Author(s):  
Stefan Neatu ◽  
Mihaela M. Trandafir ◽  
Adelina Stănoiu ◽  
Ovidiu G. Florea ◽  
Cristian E. Simion ◽  
...  

This study presents the synthesis and characterization of lanthanum-modified alumina supported cerium–manganese mixed oxides, which were prepared by three different methods (coprecipitation, impregnation and citrate-based sol-gel method) followed by calcination at 500 °C. The physicochemical properties of the synthesized materials were investigated by various characterization techniques, namely: nitrogen adsorption-desorption isotherms, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and H2–temperature programmed reduction (TPR). This experimental study demonstrated that the role of the catalytic surface is much more important than the bulk one. Indeed, the incipient impregnation of CeO2–MnOx catalyst, supported on an optimized amount of 4 wt.% La2O3–Al2O3, provided the best results of the catalytic combustion of methane on our catalytic micro-convertors. This is mainly due to: (i) the highest pore size dimensions according to the Brunauer-Emmett-Teller (BET) investigations, (ii) the highest amount of Mn4+ or/and Ce4+ on the surface as revealed by XPS, (iii) the presence of a mixed phase (Ce2MnO6) as shown by X-ray diffraction; and (iv) a higher reducibility of Mn4+ or/and Ce4+ species as displayed by H2–TPR and therefore more reactive oxygen species.


2019 ◽  
Vol 11 (1) ◽  
Author(s):  
Kaili Zhang ◽  
Xinhui Xia ◽  
Shengjue Deng ◽  
Yu Zhong ◽  
Dong Xie ◽  
...  

Abstract Controllable synthesis of highly active micro/nanostructured metal electrocatalysts for oxygen evolution reaction (OER) is a particularly significant and challenging target. Herein, we report a 3D porous sponge-like Ni material, prepared by a facile hydrothermal method and consisting of cross-linked micro/nanofibers, as an integrated binder-free OER electrocatalyst. To further enhance the electrocatalytic performance, an N-doping strategy is applied to obtain N-doped sponge Ni (N-SN) for the first time, via NH3 annealing. Due to the combination of the unique conductive sponge structure and N doping, the as-obtained N-SN material shows improved conductivity and a higher number of active sites, resulting in enhanced OER performance and excellent stability. Remarkably, N-SN exhibits a low overpotential of 365 mV at 100 mA cm−2 and an extremely small Tafel slope of 33 mV dec−1, as well as superior long-term stability, outperforming unmodified sponge Ni. Importantly, the combination of X-ray photoelectron spectroscopy and near-edge X-ray adsorption fine structure analyses shows that γ-NiOOH is the surface-active phase for OER. Therefore, the combination of conductive sponge structure and N-doping modification opens a new avenue for fabricating new types of high-performance electrodes with application in electrochemical energy conversion devices.


2020 ◽  
Vol 13 (02) ◽  
pp. 2051004
Author(s):  
Jinyan Xiong ◽  
Wei Li ◽  
Kai Zhao ◽  
Weijie Li ◽  
Gang Cheng

Nanocrystallite aggregates have great potential in semiconductor-based photocatalysis toward environmental pollution removal. In this work, we reported the fabrication of broccoli-like zinc oxide nanoaggregates in the presence of beta-cyclodextrin in ethylene glycol-H2O medium. The composition and structure of the as-obtained ZnO nanoaggregates were characterized by powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and nitrogen adsorption. It was observed that the beta-cyclodextrin played an important role in the fabrication of such broccoli-like structure. A plausible formation mechanism was discussed on the basis of the controllable experiments. The photocatalytic performance of the products was studied through the photodegradation of rhodamine B under simulated sunlight irradiation. Compared to the spherical ZnO nanoaggregates and ZnO broken spheres, the broccoli-like ZnO exhibited superior photocatalytic efficiency. Based on the photocurrent and electrochemical measurement results, the higher separation efficiency of the photogenerated carriers and lower recombination efficiency of the photoinduced electron–hole pairs over the broccoli-like ZnO nanoaggregates contributed to their remarkable photocatalytic activity.


Nanomaterials ◽  
2019 ◽  
Vol 9 (1) ◽  
pp. 100 ◽  
Author(s):  
Anton Zubrik ◽  
Marek Matik ◽  
Michal Lovás ◽  
Zuzana Danková ◽  
Mária Kaňuchová ◽  
...  

The continued decrease in water quality requires new advances in the treatment of wastewater, including the preparation of novel, effective, environmentally friendly, and affordable sorbents of toxic pollutants. We introduce a simple non-conventional mechanochemical synthesis of magnetically responsive materials. Magnetic lignite and magnetic char were prepared by high-energy ball co-milling from either raw Slovak lignite or coal-based char together with a ferrofluid. The products were characterised by X-ray diffraction, electron microscopy, 57Fe Mössbauer spectroscopy, X-ray photoelectron spectroscopy (XPS), volumetric magnetic susceptibility, and low-temperature nitrogen adsorption, and both magnetic carbons were comparatively tested as potential sorbents of As(V) oxyanions and Cd(II) cations in aqueous solutions. The magnetic char was an excellent sorbent of As(V) oxyanions (Qm = 19.9 mg/g at pH 3.9), whereas the magnetic lignite was less effective. The different sorption properties towards arsenic anions may have been due to different oxidation states of iron on the surfaces of the two magnetic composites (determined by XPS), although the overall state of iron monitored by Mössbauer spectroscopy was similar for both samples. Both magnetic composites were effective sorbents for removing Cd(II) cations (Qm (magnetic lignite) = 70.4 mg/g at pH 6.5; Qm (magnetic char) = 58.8 mg/g at pH 6.8).


1997 ◽  
Vol 04 (06) ◽  
pp. 1309-1314 ◽  
Author(s):  
D. P. FRICKEL ◽  
M. V. KUZNETSOV ◽  
E. V. SHALAEVA

X-ray photoelectron spectroscopy (XPS) and X-ray photoelectron diffraction (XPD) were used to examine the kinetics of nitrogen adsorption on the Ti(0001) surface at temperatures from 220 to 570 K and adsorption exposures from 0 to 1000 L. At the adsorption temperature T=300 K two chemically nonequivalent states of nitrogen were found: NI (1×1 lattice) localized in octapores between the first and second titanium monolayers and NII (presumably [Formula: see text] structure) on the titanium surface. The third nitrogen state, N0 , which is also localized on the surface but has unoccupied octapores in the nearest neighborhood, is observed with a decrease in the adsorption temperature to 220 K. A model of nitrogen interaction with the Ti(0001) surface in vacuum was proposed proceeding from the temperature dependence of the kinetic adsorption curves.


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